Catalyzing apparatus



April 13 1926.

D. A. LEGG ET AL CATALYZING APPARATUS Filed Feb. 20, 1923 3 Sheets-Sheet 1 nrramvsr Apfil 13, 1926. 1,580,740

D. A. LEGG ET AL CATALYZING APPARATUS" 7 Filed Feb. 20, 1923 5 Sheets-Sheet- 5 Pass A r. v13, 1926. p

UNITED STATES 1,580,740 PATENT OFFICE.

DAVID A. LEGG- AND CLARENCE W. HANCOCK, OF TERRE HAU'IE, INDIANA, ASSIGNORS T0 COMMERCIAL SOLVENTS CQRPOBATION, OF TERRE HA-UTE, INDIANA, A COR- ronarron or MARYLAND.'

} CATALYZING APPARATUS.

Application fllefi February'20, 1923. Serial No. 620,165. V

To all whom it may concern:

Be it known that we, DAVID A. LEGG and CLARENCE W. HANCOCK, both subjects of the King of Great Britain and Ireland, and residing in Terre Haute, in the county of Vigo and State of Indiana, have invented certain new and useful Improvements in Catalyzing Apparatus, of which the following is a specification, reference being made to the accompanying drawings, forming a part thereof.

Our invention relates particularly to an improved catalyzing apparatus, more par ticularly for the oxidation of the vapors of certain alcohols in the manufacture of aldehydes' The principal objects of our invention are, among other things, to provide an apparatus of this character in which exothermic or endothermic reactions in the .vapor phase requiring theuse of a catalyst, may be carried out to the best advantage, such apparatus be ing particularly adapted for endothermic and exothermic reactions in the vapor phase of which dehydrogenation and hydrogenation are typical examples.

Heretofore great difficulty has been experienced in the use of such types of apparatus to produce uniformly satisfactory" results because of inability in maintaining the constant temperatures required in the reaction chamber; such .diificulty is usually shown by marked irregularities in yields due primarily either to overheating or underheating either of the catalyst mass as a whole or of considerable portions thereof. The chief aim of our invention is therefore to provide an improved catalyzing apparatus in which the materials in vaporous form will have a free flow and ready access to the catalysts, and also to provide means Where-m. by the necessarytemperatures may be efi'ectively and uniformly maintained'throughout all portions of the catalyzer. A further object is to provide an improved means for the transfer of heat to or from the reaction chamber as required.

With these and other objects in View, our invention comprises certain novel features of construction and arrangement of parts hereinafter to be described and then particularly pointed out in the appended claims, it being understood that within the scope of such claims, various changes in form, proportion, size and inner details of construction may be made without departing from the spirit or modifying any of the advantages of the invention. \Ve liave shown our, apparatus as it has been successfully used for the dehydrogenation of normal butyl alcohol in the production of normal butyric aldehyde.

For the purpose of illustration We have shown only a single unit in the drawings, but our invention is not restricted to the use of a single unit of the apparatus hereinafter described; in fact two or more units connectedin series may be used to better advantage.

Fig. 1 is a View in elevation showing the relative location of tanks, reservoirs and catalyzer forming a part of our improved apparatus in a preferred form;

Fig. 2 is a sectional elevation taken through the center' of our improved catalyzer; v

Fig. 3 is a section taken on the line 3-3 of Fig. 2 and shows in top plan the greater portion of the catalyzing chamber;

Fig. 1 is a top plan view of the catalyzer;

' and Fig. 5 is a section taken on the line 55 of Fig. 4 and shows a saddle bracket which acts to retain the -.-atalyzing cylinder'within the container which holds the heating or cooling element depending upon the result desired.

Similar numerals refer to similar parts throughout the several figures.

Referring to Fig. 1, the reservoir 6 for the. supply of alcohol is supported on the bracket 7 and the alcohol, for example normal butyl alcohol,'fiows by gravity through the pipe 9 at a definite rate through sight feed gauge glasses 10 and by pipe 11 into a steam preheater 12 heated by steam inlet pipe 13.

Within the pre-heater 12 isthe flash boiler 14 preferably formed in a copper coil, with the copper coil 15 leading from the boiler 14 to the conduit 16. The condensed steam from the pre-heater 12 is discharged through the of spaced-apart baffles 21. Set within the cylinder 19 1s the container 22 supported on the annular bracket 23 by the circular bead 24extending from the open rim 25 of the container 22. Projecting from the sides of the container 22 are a series (five shown in Fi 2) of lateral spaced-apart ribs 26 dovetai ed between the battles 21 astshown to conserve fuel in the case of endothermic reactions. The heat is deflected as it passes upwardly through the baflie passages formed as shown by the arrows in Fig. 2. The bottom 27 of the container 22 has a like series of spaced apart ribs extending downwardly therefrom over the gas-jets 28 formed in the top of the burner 29 which is connected by the pipe 30 with any suitable source of gas supply (not shown). The cont-alner 22 acts as a support for the inner members of the catalyzer and also to hold the surrounding heating or cooling bath as required by the nature of the reaction.

Arranged concentrically within the' container 22 is the outer catalyst cylinder 31 supported by saddle brackets 32, the outer ends of which are secured to the container rim 25 by screws 33 while the inner ends of the saddle brackets 32 are likewise secured by screws to the under side of the circular lip 34 of the c linder 31, as shown in Figs. 4 and 5. Preferably'integral with the c 1 inder 31 is the inlet core 35 the upper orifice connected with the inlet pipe 18, while the lower- .end opens into va or distributing chamber'36 formed in the ower end of the cylinder31, all as shown in Fig. 2. Concentrically disposed within the cylinder 31 is the inner catalyst cylinder37 forming a surrounding annular catalyst area 38 with slotted openings 39 formed in the top flange 58 of the cylinder 37 (Fig. 4), such cylinder 37 serving as an inner wall for this catalyst area. The lower end of the cylinder 37 rests upon a cup-shaped plate 40 and against the vertical flange 41; the outer periphery of the plate 40 is supported on the annular shoulder 42 formed in the cylinder 31 along the top of the distributing chamber 36. The outer flange margin of the plate 40 is constructed as a perforated screen 43 which forms the base of the catalyst area 38 to evenly distribute the vapors passing into the catalyst area 38 as well as to prevent channeling, and also holding the catalyst material 44 from dropping into the chamber 36. The annular form of the area 38 between the cylinders 31 and 37 is a distinct advantage in maintaining the catalyst material 44 at a uniform temperature. Passing through the center of the plate 40 is the eye-bolt 45 which is removably secured to the plate 40 by nuts 46. The upper portion of the cylinder 37 is formed with a chamber 47 the side walls of which are perforated with holes 48 leading to the top of the catalyst area 38; the outlet pipe 49 is removably secured to the top plate 50 bolted to the top flange 58 of the cylinder 37 and the lip 34 of the cylinder 31 as shown, which pipe 49 carries the reaction products to the condenser 51 suitably supported on the brickwork 20 1), such condenser having the usual inlet and outlet pipes 52 and 53 for cooling water which circulates about the coil 54 within the condenser 51. The condensed products pass from the coil 54 through the pipe 55 and are caught in any suitable receiver set on the standard 57 all as shown in Fig. 1.

The circular top plate 50 rests on the flange 58 between which and the lip 34 is placed the annular gasket 59. A series of cap screws (30 removably hold the plate 50 in sealed position on the cylinder 31. The container 22 holds the heat exchanging medium 61. Any suitable hcat-exchanging medium may be employed; we have found molten solder an excellent medium for endothermic reactions, while for exothermic reactions a brine bath or other cooling medium may be used to advantage. A suitable thermometer pocket 62 carried by the bracket 63 extends downwardly within the medium 61 with the thermometer 64 projecting above the catalyzer, all as shown in Figs. 2 and 4.

The operation of our catalyzing apparatus is substantially as follows: The reacting vapors or gases from the pre-heater 12 are passed through the inlet pipe 18 and inner core 35 to the vapor distributing chamber 36 and thence upwardly through perforated screen 43 and catalystarea 38 which is filled with any suitable catalyst material 44. The reaction products pass through the holes 48 into chamber 47 and then through the outlet pipe 49 to the condenser in the usual manner, all as indicated by arrows shown in Fig. 2. During this operation the heat exchanging medium in the container 22 (Fig. 2) is maintained at a temperature favorable to the reaction, in endothermic reactions by means of the gas jets 28.

To charge the apparatus with catalyst, all the cylinders are placed within the container 22 in the positions shown in Fig. 2, except that top plate 50 is removed. The catalyst material 44 is then dropped'through the slotted openings 39 into the catalyst area 38; when this area is filled as shown in Fig. 2, the top plate 50 is replaced and fastened to the cylinder 31 by the cap-screws 60. To recharge the apparatus with fresh or revivified catalyst, the top plate .50 is removed and the inner cylinder 37 is raised and removed thereby allowing the catalyst material 44 to fall onto the plate 40 which is then withdrawn by means of the eyebolt 45. v

the units were coupled together in series and were used for the dehydrogenation of normal butyl alcohol. Heat was applied to molten solder in the container 22 by the gas jets 28 to maintain a uniform temperature in the solder throughout the run of approximately 280 C. The catalyst areaBS was charged with a suitably prepared catalyst such as is-described in United States Legg Patent No. 1,401,117 dated December 20, 1921. During the course of this run normal butyl alcohol was vaporized and tlnempreheated to 125 C. or higher after which it was passed through this pair of catalyzing units as we have shown and described. The actual amount of alcohol used was 1,254 pounds and 1,030 pounds of normal butyric aldehyde was produced which is equivalent to about 85% of the theoretical yield.

From the foregoing it is thought that the structure, operation and many advantages of our invention will be apparent to those skilled in the art without further description, and it will be understood that various changes in the size, shape, proportion and through said heat-exchanging chamber and then upwardly through saidv material.

2. In a catalyzing apparatus, an outer heat exchanging chamber, a body of catalytic material held within and against the inner'wall of said chamber in hollow cylindrical form, and means for lifting said material out of said chamber.

3. In a catalyzing apparatus, an outer heat exchanging. chamber, a hollow; cylin-.

drical body of catalytic material within. said chamber, removable means for supporting said material and holding same against the inner wall of said chamber, and means for passing vapors to be catalyzed downwardly through said heat-exchanging chamber and then introducing same into the lower portion of the catalytic material to pass upwardly therethrough. 4. In a catalyzing apparatus, an outer I heat'exchanging chamber, a body of catalytic material held within and'against the inner wall of said chamberinghollow cylindrical form, means for introducing the vapors to be catalyzed at the lower' portion bf the material, and means for lifting said material out of said chamber.

5. In a catalyzing apparatus, an outer heat exchanging chamber, an annular catalyst chamber within said heat exchanging chamber having a separable hollow core member arran ed within said catalyst chamber, a su jacent vapor distributing chamber, and a connecting member between said catalyst chamber and said distributing chamber removable from said catalyst chamber after said hollow core member has been lifted from said catalyst chamber] 6. In a catalyzing apparatus, an outer heat exchanging chamber,-an annularcatalystchamber concentrically disposed within said heat exchanging cha-mber having a separable hollow coremember arranged within said catalyst chamber, a subjacent vapor distributing chamber, and a connecting member between said catalyst and distributing chambers removable from said catalyst chamber after said hollow core member has been lifted from said catalyst chamber.

7. In a catalyzing apparatus, an outer heat exchanging chamber, an annular catavapor distributing chamber, and a, perfo rated screen between said-catalyst and dis tributing chambers removable from said catalyst chamber after said hollow core member has been lifted off said screen out of said catalyst chamber.

8. In a catalyzing apparatus, an outer heat exchanging chamber, an annular cata;

rated screen between the catalyst and dis-- tributing chambers, said screen being removable upwardly through said catalyst chamber.

10. In a catalyzing apparatus, an outer heat exchanging chamber, an annular catalyst chamber of substantially uniform width concentrically disposed within said exchanging chamber, a, vapor distributing phamber, an annular perforated screen between the catalyst and distributing chambers, said screen being removable upwardly through said catalyst chamber. 7 l

11. In a catalyzing apparatus, an outer heat exchanging chamber, a hollow cyl1ndrical body of-catalytic material within said chamber, means for supporting said material and holding same against the inner walls of said chamber, said means being removable upwardly only from said chamber.

12. In a catalyzing apparatus, an outer heat exchanging chamber, a hollow cylindrical body of catalytic material of uniform thickness within said chamber, means for supporting said material and holding same against the inner walls of said cha1nher, said means being removable upwardly only from said chamber.

13. In a catalyzing apparatus, an outer heat exchanging chamber, a hollow cylindrical body of catalytic material concentrically arranged within said chamber, means for supporting said material and hol ing same against the inner walls of said chamber, saidmeans being removable upwardly only from said chamber.

14. In a catalyzing apparatus, an outer heat exchanging chamber, a hollow cylindrical body of catalytic material of uniform thickness and concentrically arranged within said chamber, means for supporting said material and holding same against the inner Walls of said chamber, said means being removable upwardly only from said chamber. v

15. In a catalyzing apparatus, a heat exchanging chamber, an annular catalyst chamber formed in a removable cylinder disposed .within said heat exchanging chamher to hold a body of catalytic material, and means for raising said material from said catalyst chamber after said cylinder. has been lifted out of said heat exchanging chamber.

16.- In a catalyzing apparatus, a heat ex-- changing chamber, an annular catalyst chamber formed in a removable cylinder disposed concentrically Within said heat eX- changing chamber to hold a bodyof catalytic material, and means for raising said material from said catalyst chamber after said cylinder has been lifted out of said heat exchanging chamber.

l7. In a catalyzing apparatus, a heat exchanging chamber, an annular catalyst chamber formed in a cylinder disposed within said heat exchanglng chamber to hold a body of catalytic material, ayapor distributing chamber in the bottom of said cylinder, a perforated screen between said catalyst chamber and distributing chamber to support said material, and means for raising saidscreen and material out of said catalyst chamber.

18. In a catalyzing apparatus, a heat exchanging chamber, an annular catalyst chamber formed in a cylinder disposed Within said heat exchanging chamber to hold a body of catalytic material, a vapor distributing chamber in the bottom of said cylinder, a perforated screen between said catalyst chamber and distributing chamber to support said material, and detachable means for raising said screen and material out of said catalyst chamber.

19. In a catalyzing apparatus, means for preheating the vapors to be catalyzed, an

exterior chamber containing a heat exchang- I ing medium, means for heating such medium, a hollow cylindrical catalyst chamber within said medium, a vapor distributing chamber below said catalyst chamber, removable means for supporting catalytic material and holding same against the outer walls of the catalyst chamber, an inlet means for passing said preheated vapors downwardly through said medium to said dis tributing chamber, and an outlet means removably connected to said catalyst chamber adjacent said inlet means.

20. In a catalyzing apparatus, means for preheating the vapors to be catalyzed, an exterior chamber containing a heat exchanging medium, means for heating such medium, a hollow cylindrical catalyst chamber of uniform thickness concentrically disposed within said medium, a vapor distributing chamber below said catalyst chamber, removable means for supporting catalytic material and holding same against the outer Walls of the catalyst chamber, an inlet means for passing said preheated vapors downwardly through said medium to the bottom of said distributing chamber, and an outlet means removably connected to the top of said catalyst chamber adjacent said inlet means.

DAVID A. LEGG. CLARENCE W. HANCOCK. 

